反应详情

温度

160 °C

0.30 g (0.00144 mol) of 3,5-dimethoxythiophenol potassium salt was dissolved in 5 ml of 1-methyl-2-pyrrolidone, treated with 0.21 g (0.00144 mol) of 1-fluoro-4-nitrobenzene and a spatula tip of Cu powder and stirred at 160° C. for about 3 hrs. Thereafter, the solvent was removed by distillation, the residue was partitioned in water/ethyl acetate and the organic phase was washed with sat. sodium chloride solution and dried over MgSO4. After filtration and removal of the solvent the residue was chromatographed on silica gel with ethyl acetate/hexane 1:7. There was obtained 0.255 g (60%) of 1,3-dimethoxy-5-(4-nitrophenylsulphanyl)-benzene as yellow crystals; m.p.: 63-65° C.

1. customThereafter, the solvent was removed by distillation
2. customthe residue was partitioned in water/ethyl acetate
3. washthe organic phase was washed with sat. sodium chloride solution
4. dry with materialdried over MgSO4
5. filtrationAfter filtration and removal of the solvent the residue
6. customwas chromatographed on silica gel with ethyl acetate/hexane 1:7